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$X-ray Powder Diffraction in Conservation Science: Towards Routine Crystal Structure Determination of Corrosion Products on Heritage Art Objects$

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Revealing the dynamic structure of complex solid catalysts using modulated excitation X-ray diffraction.

Davide Ferri¹, Mark A Newton, Marco Di Michiel

¹Paul Scherrer Institut, 5232 Villigen PSI (Switzerland). davide.ferri@psi.ch.

Angewandte Chemie (International Ed. in English)

|June 7, 2014

Summary

Time-resolved X-ray diffraction (XRD) reveals redox dynamics of palladium nanoparticles on ceria-zirconia catalysts. This advanced technique overcomes limitations in studying low-loading precious metal catalysts.

Keywords:

X-ray diffraction ceria modulation palladium time-resolved studies

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Area of Science:

Catalysis Science
Materials Science
Surface Chemistry

Background:

X-ray diffraction (XRD) struggles to detect low loadings of finely dispersed precious metals on catalysts.
Studying redox dynamics of small nanoparticles (2 nm) on complex supports like ceria-zirconia (CZ) is challenging.

Purpose of the Study:

To investigate the redox dynamics of 2 nm palladium nanoparticles in 2 wt% Pd/CZ using time-resolved high-energy XRD.
To overcome limitations of extended X-ray absorption fine structure (EXAFS) for cerium-containing samples.

Main Methods:

Time-resolved high-energy X-ray diffraction (XRD) with a concentration modulation approach.
Synchronous diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) for surface analysis.

Main Results:

XRD successfully provided detailed redox dynamics of 2 nm Pd nanoparticles in 2 wt% Pd/CZ.
Ce maintained Pd oxidized during CO pulses; reduction occurred at the start of O2 pulses.
Oxygen transfer from Pd to Ce(3+) preceded Pd re-oxidation, with adsorbed carbonates limiting the re-oxidation rate.

Conclusions:

Time-resolved high-energy XRD is effective for studying redox dynamics of low-loading precious metal catalysts.
The study elucidated the role of the ceria-zirconia support in the catalytic cycle of palladium nanoparticles.
Adsorbed carbonates were identified as rate-limiting species in the re-oxidation process.